Microchannel Reactor for Tris-(2-chloroethyl)phosphite Synthesis

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Solution Overview

Problem

The existing methods for producing tris-(2-chloroethyl)phosphite are inefficient due to exothermic reactions in enamel reactors, leading to low aeration rates, prolonged reaction times, and side reactions that reduce the product's purity and production efficiency.

Innovation Solution

The method employs microchannel reaction technology, where phosphorus trichloride and ethylene oxide are pre-mixed and then reacted in a series of microchannel reactors with a refrigerant cooling unit, enhancing heat and mass transfer efficiency and minimizing exposure to air to prevent oxidation and hydrolysis.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If an ordinary enamel reactor is used for the esterification reaction, then the reaction can be performed with simple equipment, but the heat exchange area is very limited resulting in low aeration rate and long reaction time

Engineering Contradiction:
Improveequipment simplicityVSAvoidaeration rate
Core Design Contradiction:
Ease of manufactureVSProductivity

Solution Approach 1:

The reactor is segmented into multiple microchannel reaction units connected in series, each with small diameter channels that provide large surface area to volume ratio. This segmentation transforms the single large reactor into multiple small reaction zones, dramatically increasing the heat exchange area and enabling high aeration rates while maintaining manageable equipment complexity.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The invention transitions from a conventional three-dimensional bulk reaction space to a two-dimensional microchannel surface reaction. By utilizing the internal surface of narrow channels, the reaction occurs primarily at the interface, maximizing heat exchange area per unit volume and enabling efficient heat removal during high-rate aeration.

Inventive Principle:
Principle #17Another dimension (Dimensionality change)

2Device complexity

If the reaction is performed in an enamel reactor with limited heat exchange area, then the equipment is simple, but the reaction time is prolonged to 110 hours

Engineering Contradiction:
Improvereactor structureVSAvoidreaction time
Core Design Contradiction:
Device complexityVSDuration of action of moving object

Solution Approach 1:

The reaction process is divided into multiple stages across several microchannel reaction units connected in series. Each unit provides a controlled reaction zone with efficient heat exchange, allowing the overall reaction to proceed rapidly through sequential processing rather than requiring prolonged single-stage reaction.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The microchannel reactor enables continuous reaction process where reactants flow continuously through the series of reaction units. This continuous action eliminates idle time between reaction stages and maintains optimal reaction conditions throughout, reducing total reaction time from 110 hours to minutes.

Inventive Principle:
Principle #20Continuity of useful action

3Temperature

If the reaction system remains at 45°C-50°C for a long time, then the reaction can proceed, but side reactions occur reducing product purity to about 90%

Engineering Contradiction:
Improvereaction temperatureVSAvoidproduct purity
Core Design Contradiction:
TemperatureVSManufacturing precision

Solution Approach 1:

The microchannel reactor provides preliminary and continuous heat removal during the reaction process, preventing temperature buildup before side reactions can occur. The efficient heat exchange acts preemptively to maintain precise temperature control, eliminating the conditions that lead to oxidation and hydrolysis side reactions.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The system implements thermal feedback control where the heat generated by the exothermic reaction is immediately detected and removed through the microchannel heat exchange surfaces. This continuous feedback loop maintains temperature within the optimal range, preventing the thermal runaway that causes side reactions and purity degradation.

Inventive Principle:
Principle #23Feedback

4Duration of action of stationary object

If phosphorus trichloride is exposed to moist air for a long time, then the reaction can proceed, but oxidation and hydrolysis side reactions arise

Engineering Contradiction:
Improveexposure timeVSAvoidoxidation and hydrolysis
Core Design Contradiction:
Duration of action of stationary objectVSObject-affected harmful factors

Solution Approach 1:

The microchannel reactor system creates a closed inert environment where reactants are continuously processed without exposure to atmospheric moisture and oxygen. The rapid continuous flow through sealed microchannels eliminates the prolonged exposure to harmful atmospheric components, preventing oxidation and hydrolysis side reactions.

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This approach significantly increases the purity of tris-(2-chloroethyl)phosphite to 98% or more, while reducing reaction time from 110 hours to minutes, thereby enhancing production efficiency and product quality.

Implementation Method 1

introducing the pre-mixed mixture of the phosphorus trichloride and the ethylene oxide into a microchannel reaction device, and starting a refrigerant cooling unit of the microchannel reaction device simultaneously

Methodology Applied
Scientific EffectHeat exchange: Heat Exchanger

Implementation Method 2

The above reaction is a strong exothermic reaction

Methodology Applied
Scientific EffectExothermic reaction: Exothermic Reaction

Implementation Method 3

enhancing heat and mass transfer efficiency

Methodology Applied
Scientific EffectHeat transfer: Conduction (thermal)

Implementation Method 4

continuously pumping phosphorus trichloride and ethylene oxide into a tubular pre-mixer for pre-mixing, respectively, at a mixing pressure in a range from 0.01 MPa to 2.00 MPa, to achieve sufficient mixing

Methodology Applied
Scientific EffectMixing: Diffusion

Data Source

PatentEP2974789B1Method of preparing tris-(2-chloroethyl)phosphite
Publication Date: 2018.01.03 SHAOXING EASTLAKE HIGH TECH CO LTD
  • EP2974789B1 patent drawingFigure 1
  • EP2974789B1 patent drawingFigure 2
  • EP2974789B1 patent drawing

AI summary

The present disclosure discloses a method of preparing tris-(2-chloroethyl)phosphite, comprising: continuously pumping phosphorus trichloride and ethylene oxide into a tubular pre-mixer for pre-mixing, respectively, and starting a refrigerant cooling unit of the microchannel reaction device simultaneously, to obtain a product tris-(2-chloroethyl)phosphite after complete reaction. The method according to the present disclosure not only significantly improves the content of the esterification product, thus increasing the production efficiency by 10 to 100 times than that of an ordinary tank reactor, but also reduces the residence time of the esterification product in the reactor from 110 hours to several minutes.